関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Trichloroacetyl chloride | HCID 6420 | — |
| 反応物 | Vinyl pivalate | HCID 256591 | — |
| 反応物 | Potassium Permanganate | HCID 516875 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 生成物 | 2,2-Dichloro-3-oxocyclobutyl pivalate | HCID 57515870 | — |
反応手順
To a stirred mixture of vinyl pivalate (30 g, 234 mmol) and zinc (31 g, 468 mmol) in ether (300 ml) was added a solution of 2,2,2-trichloroacetyl chloride (55 g, 304 mmol) in ether (300 ml) dropwise (2-3 h) in a water bath. (Note: fast addition causes the reaction temp. to elevate) while maintaining the reaction temperature between 15-30° C. After the reaction was done (stained with KMnO4 solution), it was filtered through Celite. The filtrate was washed with cold water, brine, dried over MgSO4 and concentrated to give the title compound as an orange solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08633315B2 |
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| 出典データセット | uspto-grants-2014_01 |
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| ORD ID | ord-052960677a784869b91cdc966dd857ae |
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| 出典メモ | uspto-grants-2014_01 |
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